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Hydrazine → HCID 86218864, 화합물

HRID 1973194
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HRID 1973194 반응식
S(Cl)(Cl)=O.[F:5][C:6]([F:25])([F:24])[CH2:7][O:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH2:19][C:20]([F:23])([F:22])[F:21])[C:10]=1[C:11](O)=[O:12].[NH2:26][NH2:27]>CN(C)C=O.C(O)C>[F:5][C:6]([F:25])([F:24])[CH2:7][O:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH2:19][C:20]([F:23])([F:22])[F:21])[C:10]=1[C:11]([NH:26][NH2:27])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 9321HydrazineHCID 24386Thionyl ChlorideHCID 214931572,6-Bis(2,2,2-trifluoroethoxy)benzoic acid

생성물 1

HCID 86218864HCID 86218864, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 702Ethanol용매

실험 절차

Thionyl cloride (11.9 g., 100 mmole), 2,6-di(2,2,2-trifluoroethoxy)benzoic acid (2.0 g., 6.3 mmole) and two drops of dimethyl formamide are heated to reflux temperature and maintained at reflux for 4 hours. Unreacted thionyl chloride is removed by distillation on a steam bath at water aspirator pressure. The residue is dissolved in dry tetrahydrofuran and added dropwise to a solution of 95 per cent hydrazine (3.2 g., 100 mmole) in ethanol (15 ml.). The mixture is allowed to sit overnight and evaporate to dryness. The residue is diluted with water and a white solid collected and purified by sublimation (138°-140°/0.2 to 0.5 mm. Hg.) followed by recrystallization from benzene to give 2,6-di-(2,2,2-trifluoroethoxy)benzoic acid hydrazide, m.p. 153°-154° C.

후처리

  1. temperatureto reflux temperature
  2. temperaturemaintained
  3. temperatureat reflux for 4 hours
  4. customUnreacted thionyl chloride is removed by distillation on a steam bath at water aspirator pressure
  5. dissolutionThe residue is dissolved in dry tetrahydrofuran
  6. customevaporate to dryness
  7. additionThe residue is diluted with water
  8. customa white solid collected
  9. custompurified by sublimation (138°-140°/0.2 to 0.5 mm. Hg.)
  10. customfollowed by recrystallization from benzene

출처 및 근거

ORD 기록
ord-0e26af9d2fc24384adfdc8a1bd3c040f
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03996280

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